CN104725046B - A kind of 3D prints the preparation of rapid shaping zirconium-aluminium ceramic powder material - Google Patents
A kind of 3D prints the preparation of rapid shaping zirconium-aluminium ceramic powder material Download PDFInfo
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- CN104725046B CN104725046B CN201510126024.6A CN201510126024A CN104725046B CN 104725046 B CN104725046 B CN 104725046B CN 201510126024 A CN201510126024 A CN 201510126024A CN 104725046 B CN104725046 B CN 104725046B
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Abstract
The invention discloses a kind of 3D and print the preparation method of rapid shaping zirconium-aluminium ceramic powder material, it is characterized in that, first, use N (β aminoethyl) γ aminopropyl trimethoxysilane and stearic acid that zirconium-aluminium ceramic powder is carried out pretreatment, obtain pretreatment zirconium-aluminium ceramic powder；Then, in the reactor, add by mass percentage: trichloroethane: 60% ~ 70%, addition bisphenol-a polycarbonate: 2% ~ 5%, stirring and dissolving, add pretreatment zirconium-aluminium ceramic powder: 26% ~ 36%, each component sum is absolutely, it is uniformly mixed, it is placed in 50 ± 5 DEG C of constant temperature, strong stirring, back flow reaction 5 ~ 7 h, then it is spray-dried, obtain rapid shaping zirconium-aluminium ceramic powder material, this material need not spray binding agent, forming temperature can straight forming in the range of 220 ~ 230 DEG C, there is preparation technology simple, condition is easily controllable, production cost is low, it is prone to industrialized production.
Description
Technical field
The present invention relates to a kind of 3D and print the preparation method of inorganic particle moulding material, belong to the Material Field of rapid shaping, print preparation and the application of rapid shaping zirconium-aluminium ceramic powder material particularly to a kind of 3D.
Background technology
Tradition high alumina refractories improves the thermal shock resistance of material to introduce the micro-pore of structure, and so while thermal shock resistance is improved, erosion-resisting characteristics and the intensity of material suffer damage.The polycrystalline monoclinic zirconia with certain degree of aggregation is added in refractory material, the micro-crack supervened with introducing dispersion oxidation zirconium replaces the micro-pore of structure introduced in tradition anti-thermal shock refractory material design, the multiple phase refractory material that preparation thermal-shock resistance is superior, it is exactly the powder body of zirconium aluminum composite refractory, prepares variously-shaped zirconium aluminum by forming and sintering and meet pottery.
Zirconium aluminum carbon (Zr2Al3C4 and Zr3Al3C5) ceramic material is the ternary material of novel superhigh temperature resistant.They combine the advantages such as high-modulus, high rigidity, antioxidation, corrosion-resistant, high conductivity, high heat conductance, stronger destruction tolerance.Potential wide application prospect is had at high-technology fields such as Aeronautics and Astronautics, nuclear industry, superhigh temperature structural members.But as high-temperature structural material, it is widely used.Along with pottery (especially ceramic matric composite) and the development of electronics industry, require to prepare high-quality zirconium-aluminium-carbon ceramic material or the composite of complicated shape, this is that traditional molding cannot realize, variously-shaped product can be manufactured by 3D printing shaping, therefore, it is prepared as zirconium-aluminium ceramic powder material to print the material of rapid shaping, directly use 3D printer molding by 3D, reburns and form zirconium-aluminium-carbon ceramic product and will play the biggest facilitation for its application.
Rapid Prototyping technique is also known as rapid prototype manufacturing (Rapid Prototyping
Manufacturing, is called for short RPM) technology, it is born in the later stage eighties 20th century, is that a kind of high-new manufacturing technology based on material stacking method is it is considered to be manufacture a great achievement in field in recent years.It integrates mechanical engineering, CAD, reverse Engineering Technology, Layered Manufacturing Technology, Numeric Control Technology, material science, laser technology, can be changed into automatically, directly, quickly and accurately by design philosophy and there is the prototype of certain function or directly manufacture part, thus provide the realization rate of a kind of high efficiency, low cost for the aspect such as verification of part prototype, new design philosophy.That is, Rapid Prototyping technique is exactly the data utilizing 3DCAD, by rapidform machine, material stacking from level to level is become physical prototypes.3D prints (Three Dimonsion
Printing, is called for short 3DP) it is a kind of rapid shaping technique, the 3D model data of Computer Design can being divided into synusia model data, specific raw materials in layer being piled up molding until completing the structure of whole entity.3DP molding has the advantages such as low cost, work process is pollution-free, shaping speed is fast.
null3D printing technique has 3DP technology、FDM fusion stacking forming technique、SLA stereolithography techniques、SLS precinct laser sintering、DLP laser formation technology and UV ultraviolet forming technique，Technology difference material therefor is the most entirely different，The most often FDM3D printing technique applied with our ordinary people and family，This technology can enter into family，Simple to operate，Material therefor is generally easy to get，This technology prints the product the articles for daily use also close to us，Material used is mainly environmental protection macromolecule material，As: PLA、PCL、PHA、PBS、PA、ABS、PC、PS、PVC，Because this technology is to print the most on the table，Abnormal smells from the patient produced by melted macromolecular material or decomposition produce harmful substance and directly contact with our people，Easily cause safety problem.Industrial parts etc. need the material that the product of some strength function can select to adapt.
In existing moulding material field, owing to SLS rapid shaping technique has the advantages such as raw material sources various and part structure time is shorter, therefore there is wide application in rapid shaping field.Chinese invention patent CN1379061A discloses a kind of nylon powder body material for laser sintering and moulding goods, by chemosynthesis and the improvement of technique, the surface of nylon powder body material is processed, obtain sintering character excellent, moulded products intensity is high, the product of good toughness, simplifies the preparation technology of laser sintered nylon material, reduces cost.But SLS technique also exists many deficiencies and seriously limits the application further of SLS and popularize；Thus also make to be restricted based on SLS technological forming materials'use.
3DP technique is similar with SLS technique, all use the molding of powder body material constituency, except that the powder body material of 3DP technique couples together not by the sintering layer by layer of laser, but under the effect of shower nozzle, with bonding agent (such as silica gel), the cross section information of part " is printed " on powder body material.Owing to 3DP is by sprinkler bonding agent molding, it is to avoid use using and promoting of the use cost of the agglomerating plant of the complex and expensive such as laser, beneficially rapid shaping technique.Chinese invention patent CN102093646 B discloses a kind of preparation method printing rapid prototyping material for 3D, is powder body material to be carried out a series of modification obtain modified powder materials A, modified powder materials A and bonding agent B adapted during use.
The present invention is modified by powder body material carries out Dispersion on surface, obtains Superfine Zirconium aluminium ceramic powder material and can reach micron order even submicron order, and the powder body material of uniform particle diameter；Starting with from powder-modified formula, the powder body inorganic material obtained under certain temperature and pressure can straight forming, it is not necessary to sprays bonding agent, is greatly simplified program of just doing.Obtained by product not only formed precision high, also make thin-walled micro parts be molded on 3DP rapidform machine be implemented as possibility；Additionally, the method that this patent provides is simple, low cost.
Summary of the invention
The mesh of the present invention is to provide a kind of 3D and prints the preparation method of rapid shaping zirconium-aluminium ceramic powder material, and rapid shaping powder body need not spray binding agent can straight forming；
The purpose of the present invention is achieved through the following technical solutions.
A kind of 3D prints the preparation method of rapid shaping zirconium-aluminium ceramic powder material, is characterised by that the method has a following processing step:
(1) zirconium-aluminium ceramic powder pretreatment: in grinder, add by mass percentage, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane: 5% ~ 12%, stearic acid: 2% ~ 10%, zirconium-aluminium ceramic powder: 80% ~ 90%, each component sum is absolutely, opens grinder rotating speed at 300 revs/min, grinding at room temperature 0.5 ~ 1.5 h, obtains pretreatment zirconium-aluminium ceramic powder；
(2) 3D prints the preparation of rapid shaping zirconium-aluminium ceramic powder material: in the reactor, add by mass percentage: trichloroethane: 60% ~ 70%, addition bisphenol-a polycarbonate: 2% ~ 5%, stirring and dissolving, add pretreatment zirconium-aluminium ceramic powder: 26% ~ 36%, each component sum is absolutely, it is uniformly mixed, it is placed in 50 ± 5 DEG C of constant temperature, strong stirring, back flow reaction 5 ~ 7 h, then it is spray-dried, obtain rapid shaping zirconium-aluminium ceramic powder material, it is in the range of 1.0 ~ 2.5 μm that obtained 3D prints the particle diameter of rapid shaping zirconium-aluminium ceramic powder material.
The particle diameter of zirconium-aluminium ceramic powder described in step (1) is in 0.8 ~ 2.0 μ m；
Spray drying described in step (2), inlet temperature controls in the range of 60 ~ 70 DEG C, trichloroethane recycling.
Particle size test method of the present invention is the granularity equivalent diameter size using laser particle analyzer to record.
It is a further object of the present invention to provide a kind of for 3D printing rapid shaping powder body material application of molding on 3D printer, feature is: takes rapid shaping powder body material and is placed on 3D printing rapidform machine, on the horizontal plane X sprawling uniform rapid shaping powder body material and Y-direction (X and Y-direction represent the horizontal and vertical of horizontal plane respectively), in the vertical Z-direction of plane, then decline certain altitude.Again next layer being carried out rapid shaping powder body material to sprawl, so repeat, after all having fed, temperature can straight forming in the range of being raised to 220 ~ 230 DEG C.
The present invention compared with the prior art, has the advantage that and beneficial effect:
(1) present invention obtains 3D and prints rapid shaping zirconium-aluminium ceramic powder material, it is not necessary to spraying binding agent can straight forming in the range of heating 220 ~ 230 DEG C.
(2) present invention obtains 3D and prints rapid shaping zirconium-aluminium ceramic powder material, and granule can reach submicron order even nanoscale, has meso-position radius grain little, the feature that particle size distribution is narrow, stable in properties；Thin-walled model or small parts can be manufactured by this rapid shaping powder body material, produce product and there is formed precision high feature.
(3) present invention obtains 3D and prints rapid shaping zirconium-aluminium ceramic powder material, has preparation technology simple, and condition is easily controllable, and production cost is low, it is easy to industrialized production.
(4) present invention obtains 3D and prints rapid shaping zirconium-aluminium ceramic powder material, it is possible to effective rapid shaping on 3D printer, can be applicable to the 3D printer of multiple different model.
Detailed description of the invention
Embodiment 1
(1) zirconium-aluminium ceramic powder pretreatment: in grinder, it is separately added into, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane: 8 mL, stearic acid: 5g, zirconium-aluminium ceramic powder: 87g, open grinder rotating speed at 300 revs/min, grinding at room temperature 1 h, obtain pretreatment zirconium-aluminium ceramic powder；
(2) 3D prints the preparation of rapid shaping zirconium-aluminium ceramic powder material: in the reactor, it is separately added into: trichloroethane: 45 mL, add bisphenol-a polycarbonate: 3g, stirring and dissolving, add pretreatment zirconium-aluminium ceramic powder: 32g, it is uniformly mixed, it is placed in 50 DEG C of constant temperature, strong stirring, back flow reaction 6 h, then it is spray-dried, obtaining rapid shaping zirconium-aluminium ceramic powder material, it is in the range of 1.0 ~ 2.5 μm that obtained 3D prints the particle diameter of rapid shaping zirconium-aluminium ceramic powder material.
Embodiment 2
(1) zirconium-aluminium ceramic powder pretreatment: in grinder, it is separately added into, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane: 10 mL, stearic acid: 10g, zirconium-aluminium ceramic powder: 80g, open grinder rotating speed at 300 revs/min, grinding at room temperature 0.5 h, obtain pretreatment zirconium-aluminium ceramic powder；
(2) 3D prints the preparation of rapid shaping zirconium-aluminium ceramic powder material: in the reactor, it is separately added into: trichloroethane: 48 mL, add bisphenol-a polycarbonate: 5g, stirring and dissolving, add pretreatment zirconium-aluminium ceramic powder: 26g, it is uniformly mixed, it is placed in 55 DEG C of constant temperature, strong stirring, back flow reaction 5 h, then it is spray-dried, obtaining rapid shaping zirconium-aluminium ceramic powder material, it is in the range of 1.0 ~ 2.5 μm that obtained 3D prints the particle diameter of rapid shaping zirconium-aluminium ceramic powder material.
Embodiment 3
(1) zirconium-aluminium ceramic powder pretreatment: in grinder, it is separately added into, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane: 7 mL, stearic acid: 3g, zirconium-aluminium ceramic powder: 90g, open grinder rotating speed at 300 revs/min, grinding at room temperature 1.5 h, obtain pretreatment zirconium-aluminium ceramic powder；
(2) 3D prints the preparation of rapid shaping zirconium-aluminium ceramic powder material: in the reactor, it is separately added into: trichloroethane: 46 mL, add bisphenol-a polycarbonate: 4g, stirring and dissolving, add pretreatment zirconium-aluminium ceramic powder: 30g, it is uniformly mixed, it is placed in 45 DEG C of constant temperature, strong stirring, back flow reaction 7 h, then it is spray-dried, obtaining rapid shaping zirconium-aluminium ceramic powder material, it is in the range of 1.0 ~ 2.5 μm that obtained 3D prints the particle diameter of rapid shaping zirconium-aluminium ceramic powder material.
Embodiment 4
(1) zirconium-aluminium ceramic powder pretreatment: in grinder, it is separately added into, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane: 12mL, stearic acid: 2g, zirconium-aluminium ceramic powder: 86g, open grinder rotating speed at 300 revs/min, grinding at room temperature 1.2 h, obtain pretreatment zirconium-aluminium ceramic powder；
(2) 3D prints the preparation of rapid shaping zirconium-aluminium ceramic powder material: in the reactor, it is separately added into: trichloroethane: 42 mL, add bisphenol-a polycarbonate: 4g, stirring and dissolving, add pretreatment zirconium-aluminium ceramic powder: 36g, it is uniformly mixed, it is placed in 52 DEG C of constant temperature, strong stirring, back flow reaction 5.5 h, then it is spray-dried, obtaining rapid shaping zirconium-aluminium ceramic powder material, it is in the range of 1.0 ~ 2.5 μm that obtained 3D prints the particle diameter of rapid shaping zirconium-aluminium ceramic powder material.
Embodiment 5
(1) zirconium-aluminium ceramic powder pretreatment: in grinder, it is separately added into, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane: 10mL, stearic acid: 8g, zirconium-aluminium ceramic powder: 82g, open grinder rotating speed at 300 revs/min, grinding at room temperature 0.8 h, obtain pretreatment zirconium-aluminium ceramic powder；
(2) 3D prints the preparation of rapid shaping zirconium-aluminium ceramic powder material: in the reactor, it is separately added into: trichloroethane: 44 mL, add bisphenol-a polycarbonate: 2g, stirring and dissolving, add pretreatment zirconium-aluminium ceramic powder: 34g, it is uniformly mixed, it is placed in 48 DEG C of constant temperature, strong stirring, back flow reaction 6.5 h, then it is spray-dried, obtaining rapid shaping zirconium-aluminium ceramic powder material, it is in the range of 1.0 ~ 2.5 μm that obtained 3D prints the particle diameter of rapid shaping zirconium-aluminium ceramic powder material.
Embodiment 6
(1) zirconium-aluminium ceramic powder pretreatment: in grinder, it is separately added into, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane: 5mL, stearic acid: 7g, zirconium-aluminium ceramic powder: 88g, open grinder rotating speed at 300 revs/min, grinding at room temperature 1 h, obtain pretreatment zirconium-aluminium ceramic powder；
(2) 3D prints the preparation of rapid shaping zirconium-aluminium ceramic powder material: in the reactor, it is separately added into: trichloroethane: 50 mL, add bisphenol-a polycarbonate: 2g, stirring and dissolving, add pretreatment zirconium-aluminium ceramic powder: 28g, it is uniformly mixed, it is placed in 50 DEG C of constant temperature, strong stirring, back flow reaction 6 h, then it is spray-dried, obtaining rapid shaping zirconium-aluminium ceramic powder material, it is in the range of 1.0 ~ 2.5 μm that obtained 3D prints the particle diameter of rapid shaping zirconium-aluminium ceramic powder material.
Using method: in Example, the rapid shaping powder body material of synthesis is placed on 3D printing rapidform machine, on the horizontal plane X sprawling uniform rapid shaping powder body material and Y-direction (X and Y-direction represent the horizontal and vertical of horizontal plane respectively), in the vertical Z-direction of plane, then decline certain altitude.Again next layer being carried out rapid shaping powder body material to sprawl, so repeat, after all having fed, temperature can straight forming in the range of being raised to 220 ~ 230 DEG C.
Claims (4)
1. a 3D prints the preparation method of rapid shaping zirconium-aluminium ceramic powder material, it is characterised in that the method have with
Lower processing step:
(1) zirconium-aluminium ceramic powder pretreatment: in grinder, adds by mass percentage, N-(β-aminoethyl)-γ-ammonia third
Base trimethoxy silane: 5%～12%, stearic acid: 2%～10%, zirconium-aluminium ceramic powder: 80%～90%, each component sum is
Absolutely, open grinder rotating speed at 300 revs/min, grinding at room temperature 0.5～1.5h, obtain pretreatment zirconium-aluminium ceramic powder；
(2) 3D prints the preparation of rapid shaping zirconium-aluminium ceramic powder material: in the reactor, adds by mass percentage: three
Ethyl chloride: 60%～70%, addition bisphenol-a polycarbonate: 2%～5%, stirring and dissolving, add pretreatment zirconia-alumina-carbon ceramic powder
Body: 26%～36%, each component sum is absolutely, is uniformly mixed, and is placed in 50 ± 5 DEG C of constant temperature, strong stirring, returns
Stream reaction 5～7h, is then spray-dried, and obtains rapid shaping zirconium-aluminium ceramic powder material, and obtained 3D prints fast rapid-result
The particle diameter of type zirconium-aluminium ceramic powder material is in the range of 1.0～2.5 μm.
A kind of 3D the most according to claim 1 prints the preparation method of rapid shaping zirconium-aluminium ceramic powder material, its feature
Being, the spray drying described in step (2), inlet temperature controls in the range of 60～70 DEG C.
A kind of 3D the most according to claim 1 prints the preparation method of rapid shaping zirconium-aluminium ceramic powder material, its feature
It is, the solvent trichloroethane recycling in the spray drying described in step (2).
A kind of 3D the most according to claim 1 prints prepared by the preparation method of rapid shaping zirconium-aluminium ceramic powder material
3D prints rapid shaping zirconium-aluminium ceramic powder material, it is characterised in that 3D prints rapid shaping zirconium-aluminium ceramic powder material and exists
Forming temperature rapid shaping in the range of 220～230 DEG C on three-dimensional printer.
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| CA3039691A1 (en) * | 2015-10-09 | 2017-04-13 | Syddansk Universitet | Feedstock for 3d printing and uses thereof |
| CN105601287B (en) * | 2015-12-24 | 2018-03-30 | 湖南世纪特邦新材料有限公司 | A kind of 3D printing ceramic material binding agent and its application |
| CN106147172A (en) * | 2016-07-29 | 2016-11-23 | 苏州秉创科技有限公司 | A kind of 3D printing consumables being easy to secondary plasticity |
| CN106147174A (en) * | 2016-07-29 | 2016-11-23 | 苏州秉创科技有限公司 | A kind of 3D printing consumables being prone to degraded |
| US10954377B2 (en) | 2016-09-26 | 2021-03-23 | Sabanci Üniversitesi | Admixture and ink comprising the admixture |
| CN108046757A (en) * | 2017-12-20 | 2018-05-18 | 长沙市西欧电子科技有限公司 | A kind of preparation method of high performance 3 d printing composite material |
| CN112457003B (en) * | 2020-12-16 | 2021-12-21 | 华南理工大学 | Novel BT/HA biphase piezoelectric biological ceramic bone tissue engineering restoration and preparation method thereof |
| WO2022265610A1 (en) | 2021-06-18 | 2022-12-22 | Sabanci Universitesi | Preparation of ceramic doughs through coagulation, for green machining |
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| CN103936428A (en) * | 2014-03-13 | 2014-07-23 | 济南大学 | Preparation method of rapid molding powder material used for three dimensional printing |
| CN103980397A (en) * | 2014-04-30 | 2014-08-13 | 中国科学院化学研究所 | 3D printing composition, preparation and application methods and product thereof |
| CN104291338A (en) * | 2014-09-10 | 2015-01-21 | 济南大学 | Preparation method of rapid-prototyping nano-silicon carbide material for 3D printing |
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| US6733703B2 (en) * | 2000-09-26 | 2004-05-11 | Romain L. Billiet | Method for controlling the dimensions of bodies made from sinterable materials |
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| CN103936428A (en) * | 2014-03-13 | 2014-07-23 | 济南大学 | Preparation method of rapid molding powder material used for three dimensional printing |
| CN103980397A (en) * | 2014-04-30 | 2014-08-13 | 中国科学院化学研究所 | 3D printing composition, preparation and application methods and product thereof |
| CN104291338A (en) * | 2014-09-10 | 2015-01-21 | 济南大学 | Preparation method of rapid-prototyping nano-silicon carbide material for 3D printing |
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